EP4287342A1 - Procédé de fabrication d'électrolyte solide pour batterie à électrolyte solide - Google Patents

Procédé de fabrication d'électrolyte solide pour batterie à électrolyte solide Download PDF

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Publication number
EP4287342A1
EP4287342A1 EP23159113.2A EP23159113A EP4287342A1 EP 4287342 A1 EP4287342 A1 EP 4287342A1 EP 23159113 A EP23159113 A EP 23159113A EP 4287342 A1 EP4287342 A1 EP 4287342A1
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EP
European Patent Office
Prior art keywords
solid electrolyte
lithium
ceramic
solid
over
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP23159113.2A
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German (de)
English (en)
Inventor
Miriam Kunze
Stephan Leonhard Koch
Tobias JANSEN
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Volkswagen AG
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Volkswagen AG
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Filing date
Publication date
Application filed by Volkswagen AG filed Critical Volkswagen AG
Publication of EP4287342A1 publication Critical patent/EP4287342A1/fr
Pending legal-status Critical Current

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
    • H01M10/0562—Solid materials
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G25/00—Compounds of zirconium
    • C01G25/006—Compounds containing, besides zirconium, two or more other elements, with the exception of oxygen or hydrogen
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/058—Construction or manufacture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/44—Methods for charging or discharging
    • H01M10/446—Initial charging measures
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0017—Non-aqueous electrolytes
    • H01M2300/0065—Solid electrolytes
    • H01M2300/0068—Solid electrolytes inorganic
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0017—Non-aqueous electrolytes
    • H01M2300/0065—Solid electrolytes
    • H01M2300/0068—Solid electrolytes inorganic
    • H01M2300/0071—Oxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/04—Processes of manufacture in general
    • H01M4/0438—Processes of manufacture in general by electrochemical processing
    • H01M4/044—Activating, forming or electrochemical attack of the supporting material
    • H01M4/0445—Forming after manufacture of the electrode, e.g. first charge, cycling
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the invention relates to a method for producing a solid electrolyte for a solid battery and a battery cell with such a solid electrolyte.
  • Rechargeable electrochemical storage systems are becoming increasingly important for many areas of daily life.
  • High-capacity energy storage devices such as lithium-ion (Li-ion) batteries and capacitors
  • Li-ion lithium-ion
  • UPS uninterruptible power supply
  • the charge/discharge time and the capacity of energy storage devices are the crucial parameters.
  • the size, weight and/or cost of such energy storage devices are also important parameters.
  • low internal resistance is required for high performance. The lower the resistance, the fewer restrictions the energy storage device faces when delivering electrical energy.
  • Li-ion batteries are said to best achieve the desired capacity and the desired cycling.
  • Li-ion batteries in their current form often lack the energy capacity and number of charge/discharge cycles for these growing applications.
  • lithium-ion batteries are widely used today. In consumer electronics, for example, they are used in portable devices such as cell phones and smartphones, laptops and tablets, etc.
  • lithium-ion batteries are an important component of electric vehicles, as electric batteries are used in electric cars and hybrid vehicles and have therefore become part of mass production.
  • Solid-state batteries which are already close to being ready for series production and offer many advantages for use in electric cars.
  • Solid-state batteries offer advantages over well-known lithium-ion batteries a higher energy density, the batteries can therefore be made smaller or more powerful with the same size, offer even more safety and can be charged faster.
  • solid-state batteries do not require a cooling circuit, as is necessary for lithium-ion batteries with liquid electrolyte. This saves space and weight. They can achieve significantly more charging cycles, do not self-decompose or overheat and offer a more homogeneous power distribution. They can also be built with very thin electrolyte layers that are also flexible.
  • a lithium-based solid cell which has a cell stack made of a copper substrate, a graphite layer, a solid electrolyte and a nickel-manganese-cobalt oxide layer.
  • the solid electrolyte is in contact with the graphite layer and with the nickel-manganese-cobalt oxide layer.
  • the copper substrate forms an anode of the cell stack and the nickel-manganese-cobalt oxide layer forms a cathode of the cell stack. It is envisaged that the solid electrolyte is a lithium-based electrolyte.
  • the graphite layer has a first SEI (solid electrolyte interface) and a second electrolyte interface that is achieved during pre-lithiation with a liquid lithium-based electrolyte, and a second SEI that is achieved during pre-lithiation with the polymeric lithium-based electrolyte.
  • a method for producing a dry electrode for a solid-state battery in which an electrode material comprising an active substance, a conductive material, a first solid electrolyte material and a first binder is processed into an electrode film by dry film production.
  • the US 2019/0 372 127 A1 describes a cell, which is a hybrid of a battery cell and a capacitor.
  • the cell includes a porous anode and a porous cathode made of a lithium compound.
  • the cathode is electrically connected to the capacitor.
  • a liquid electrolyte is used to enable electron transport from the anode to the cathode.
  • the invention is based on the object of further increasing the energy density and the service life of a solid-state battery.
  • an over-lithiated solid electrolyte is to be understood as meaning a solid electrolyte that has more lithium than intended in the stoichiometric ratio of the solid electrolyte.
  • an over-lithiated solid electrolyte is to be understood as meaning a solid electrolyte which has at least 1 mol% more lithium, preferably at least 3 mol%, particularly preferably at least 5 mol% more lithium than a stoichiometric solid electrolyte.
  • the method makes it possible to deposit a higher amount of lithium in a solid-state battery in which an anode is formed in situ in the first charging cycle and thus increase the capacity of the solid-state battery.
  • the cathode can be dimensioned smaller in order to provide sufficient lithium for the deposition of an anode formed in situ, since additional lithium is provided by the over-lithiated solid electrolyte. This allows the weight of the solid-state battery to be reduced.
  • the smaller dimensions of the cathode can also save raw materials and the associated costs.
  • the risk of lithium depletion at the cathode is reduced, which can increase the life of the battery cell of the solid-state battery.
  • lithium losses can occur at the anode formed in situ through side reactions. These losses can be compensated for by over-lithiation of the solid electrolyte.
  • the "reserve lithium" from over-lithiation reacts in place of the anode's active lithium.
  • the term “ceramic-specific stoichiometric ratio” is understood to mean the molar proportions of the elements involved, which are predetermined by the valences and oxidation states of the elements involved, for a ceramic composition that is overall uncharged.
  • the ceramic solid electrolyte for over-lithiation in particular a ceramic membrane
  • the ceramic solid electrolyte, in particular the ceramic membrane is immersed in molten lithium.
  • the ceramic solid electrolyte, in particular the ceramic membrane is preferably immersed in molten lithium after a sintering process.
  • a solid electrolyte powder can be mixed with lithium powder to produce the solid electrolyte and then the mixture can be heated to a temperature of 180 ° C - 300 ° C, whereby the lithium powder melts.
  • a ceramic membrane would be made from the solid electrolyte only after loading with the additional lithium from the molten lithium powder.
  • the solid electrolyte powder as a starting material for producing a solid electrolyte and the powder can also be ground together to create a starting material which is suitable for producing an over-lithiated solid electrolyte.
  • Another preferred option for over-lithiation of the solid electrolyte is to vapor deposition or sputter a lithium layer onto the ceramic solid electrolyte and then heat the solid electrolyte with the vapor deposited or sputtered lithium layer so that the free lithium from the applied layer in the Solid electrolyte is absorbed.
  • the over-lithiation takes place at a temperature of 180 ° C to 300 ° C. In this temperature range, elemental lithium exists in a liquid state, while the temperature is low enough to avoid decomposition or other damage to the ceramic solid electrolyte. As a result, over-lithiation of the solid electrolyte can be achieved in a particularly simple and energy-saving manner.
  • the lithium concentration of the ceramic is increased by an electrochemical process.
  • the solid electrolyte is coated with lithium and a liquid electrolyte is applied. An electrical potential is then applied and the lithium goes into the solid electrolyte.
  • the process can also be carried out without applying an additional electrical potential, in which case the lithium transfers into the solid electrolyte due to the potential that forms itself in accordance with the electrochemical voltage series.
  • the solid electrolyte has a NASICON structure, with the additional lithium being incorporated into interstitial sites in the crystal structure of the solid electrolyte.
  • Suitable lithium-analog structures from NASICON include, in particular, lithium phosphates of the formula LiM 2 (PO 4 ) 3 , where M represents a base element selected from the group Ti, Ge, Zr, Hf or Sn.
  • the lithium phosphates can be doped, with Al, Cr, Ga, Fe, Sc, In, Lu, Y and La preferably serving as dopant.
  • LAGP Li 1.4 Al 0.4 Ge 0.2 Ti 1.6 (PO 4 ) 3 LAGTP.
  • the excess lithium is deposited in situ when the cell is first charged to form an anode.
  • a correspondingly strong over-lithiation of the solid electrolyte is necessary.
  • a portion of the lithium can be introduced into the battery cell by dimensioning the cathode appropriately.
  • By over-lithiating the solid electrolyte significantly more lithium can be introduced into the battery cell, so that the cathode can be made smaller. This means that less material is required overall, so that gravimetric and volume-specific energy density of the battery cell can be increased. The additional lithium settles at defective locations in the crystal structure as well as at interstitial sites.
  • the over-lithiation and the additional lithium on the one hand increase the conductivity for lithium ions and on the other hand make free lithium available, which is deposited in situ as anode material during the first charging process of the battery cell and thus forms the anode of the battery cell.
  • the solid electrolyte has a LISICON structure, with the additional lithium being incorporated into interstitial sites in the crystal structure of the solid electrolyte.
  • LISICON is an acronym for Lithium Super lonic Conductor and originally referred to a family of minerals with the chemical formula Li 2+2x Zn 1-x GeO 4 .
  • Solid electrolytes with a LISICON structure also enable additional absorption of lithium, so that these solid electrolytes can also be over-lithiated and thus provide additional lithium for the function in the battery cell of a solid-state battery.
  • the solid electrolyte has a garnet structure, with the additional lithium being incorporated into interstitial sites in the crystal structure of the solid electrolyte.
  • garnets are orthosilicates with the general composition X 3 Y 2 (SiO 4 ) 3 , which crystallize in the cubic crystal system, where The individual SiO 4 tetrahedra are connected to each other by ionic bonds via the interstitial B cations.
  • Garnet-like compounds with an excess of lithium are good lithium ion conductors.
  • ionic conductors with a garnet-like structure are lithium lanthanum zirconium oxide Li 7 La 3 Zr 2 O 12 (LLZO), Li 6.25 La 3 Zr2AL 0.25 O 12 lithium lanthanum zirconium aluminate and lithium lanthanum zirconium tantalate Li 6.6 La 3 Zr 1.6 Ta 0.4 O 12 .
  • LLZO lithium lanthanum zirconium oxide
  • Li 6.25 La 3 Zr2AL 0.25 O 12 lithium lanthanum zirconium aluminate
  • lithium lanthanum zirconium tantalate Li 6.6 La 3 Zr 1.6 Ta 0.4 O 12 .
  • over-lithiation leads to a ratio of Li 7.5 La 3 Zr 2 O 12 with a 1mol% over-lithiation to a ratio of Li 8 La 3 Zr 2 O 12 with a 3mol% over-lithiation and of Li 9 La 3 Zr 2 O 12 with a 5mol% over-lithiation.
  • LLZO lithium lanthanum zirconium oxide
  • the solid electrolyte has a perovskite structure or anti-perovskite structure, whereby the additional lithium is incorporated into interstitial sites in the crystal structure of the solid electrolyte.
  • a particularly suitable representative of perovskites is lithium lanthanum titanate (LLTO), with vacancies in the perovskite structure enabling high conductivity.
  • Solid electrolytes with a perovskite structure also enable additional absorption of lithium, so that these solid electrolytes can also be over-lithiated and thus provide additional lithium for the function in the battery cell of a solid-state battery.
  • a further aspect of the invention relates to a solid electrolyte for use in a solid state battery, the solid electrolyte being over-lithiated using one of the methods described in the preceding sections.
  • a battery cell with such a solid electrolyte enables a higher energy density with the same size compared to the battery cells known from the prior art or a smaller size with the same energy density.
  • the cathode can be dimensioned smaller in order to provide sufficient lithium for the deposition of an anode formed in situ, since additional lithium is provided by the over-lithiated solid electrolyte. This allows the weight of the solid-state battery to be reduced.
  • the smaller dimensions of the cathode can also save raw materials and the associated costs.
  • lithium depletion at the cathode is reduced, which can increase the life of the battery cell of the solid-state battery.
  • lithium losses can occur at the anode formed in situ through side reactions. These losses can be compensated for by over-lithiation of the solid electrolyte.
  • the "reserve lithium" from over-lithiation reacts in place of the anode's active lithium oxide.
  • FIG. 1 shows a schematic representation of the production of a battery cell 12 for a solid-state battery 10.
  • the battery cell 12 comprises a cathode 14 and a ceramic solid electrolyte 16, 18, which is overcharged with lithium 22 by a process for over-lithiation compared to the stoichiometric ratio of the ceramic 18.
  • the battery cell 12 is designed to form an anode 28 in situ on a side of the solid electrolyte 16 facing away from the cathode 14.
  • the ceramic 18 is immersed in an immersion bath 20 with molten lithium 22.
  • the immersion bath 20 has a heating element 24 and a control unit 26, with which in particular the temperature of the molten lithium 22 in the immersion bath 20 can be controlled.
  • the solid electrolyte 16 can be overcharged with lithium 22, so that more lithium 22 is present in the solid electrolyte 16 than the stoichiometric composition of the ceramic 18 provides. This makes it possible to produce a mechanically stable solid electrolyte 16, which can provide additional free lithium 22 for the formation of an anode.
  • the molten lithium 22 in the immersion bath 20 preferably has a temperature which is above the melting point of lithium 22 at 180 ° C and below 300 ° C in order to avoid decomposition or other thermal or chemical damage to the ceramic 18 of the solid electrolyte 16 .
  • FIG 2 a flow chart for producing a solid electrolyte 16 according to the invention is shown.
  • the ceramic solid electrolyte 16 is formed, which can be done in particular by a sintering process, whereby the ceramic 18 of the solid electrolyte 16 is produced with a desired stoichiometric ratio of the elements used.
  • the ceramic 18 is cooled until the solid electrolyte 16 has reached its desired mechanical strength.
  • the solid electrolyte 16 is over-lithiated by introducing additional lithium into the lattice structure of the ceramic solid electrolyte 16.
  • the over-lithiated solid electrolyte 16 is then removed from the process environment for incorporating lithium atoms into the ceramic 18 in a process step ⁇ 130> and fed to a process for producing a cell stack for the battery cell 12.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Physics & Mathematics (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Secondary Cells (AREA)
  • Conductive Materials (AREA)
EP23159113.2A 2022-05-31 2023-02-28 Procédé de fabrication d'électrolyte solide pour batterie à électrolyte solide Pending EP4287342A1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE102022205467.9A DE102022205467B3 (de) 2022-05-31 2022-05-31 Verfahren zur Herstellung eines Feststoffelektrolyts für eine Feststoffbatterie

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EP4287342A1 true EP4287342A1 (fr) 2023-12-06

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EP23159113.2A Pending EP4287342A1 (fr) 2022-05-31 2023-02-28 Procédé de fabrication d'électrolyte solide pour batterie à électrolyte solide

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EP (1) EP4287342A1 (fr)
KR (1) KR20230166916A (fr)
CN (1) CN117154193A (fr)
DE (1) DE102022205467B3 (fr)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110233298A (zh) * 2019-07-09 2019-09-13 珠海冠宇电池有限公司 一种新型全固态锂离子电池的制备方法
US20190372127A1 (en) 2018-06-01 2019-12-05 GM Global Technology Operations LLC Pre-lithiation of anodes for high performance capacitor assisted battery
CN113381055A (zh) * 2020-03-10 2021-09-10 中国科学院上海硅酸盐研究所 一种低界面阻抗的锂/石榴石基固态电解质界面及其制备方法
CN113571672A (zh) 2021-07-26 2021-10-29 中汽创智科技有限公司 一种干法电极、固态锂离子电池及其制备方法
WO2022008506A1 (fr) 2020-07-10 2022-01-13 Renault S.A.S Cellule au lithium solide, batterie comprenant lesdites cellules et procédé de fabrication pour fabriquer ladite batterie

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20190372127A1 (en) 2018-06-01 2019-12-05 GM Global Technology Operations LLC Pre-lithiation of anodes for high performance capacitor assisted battery
CN110233298A (zh) * 2019-07-09 2019-09-13 珠海冠宇电池有限公司 一种新型全固态锂离子电池的制备方法
CN113381055A (zh) * 2020-03-10 2021-09-10 中国科学院上海硅酸盐研究所 一种低界面阻抗的锂/石榴石基固态电解质界面及其制备方法
WO2022008506A1 (fr) 2020-07-10 2022-01-13 Renault S.A.S Cellule au lithium solide, batterie comprenant lesdites cellules et procédé de fabrication pour fabriquer ladite batterie
CN113571672A (zh) 2021-07-26 2021-10-29 中汽创智科技有限公司 一种干法电极、固态锂离子电池及其制备方法

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Publication number Publication date
KR20230166916A (ko) 2023-12-07
CN117154193A (zh) 2023-12-01
DE102022205467B3 (de) 2023-08-31

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